CN105112036B - Barium strontium calcium descaling and blockage relieving agent and preparation method thereof near wellbore zone - Google Patents
Barium strontium calcium descaling and blockage relieving agent and preparation method thereof near wellbore zone Download PDFInfo
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- CN105112036B CN105112036B CN201510521958.XA CN201510521958A CN105112036B CN 105112036 B CN105112036 B CN 105112036B CN 201510521958 A CN201510521958 A CN 201510521958A CN 105112036 B CN105112036 B CN 105112036B
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
- C09K8/528—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning inorganic depositions, e.g. sulfates or carbonates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating
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Abstract
The barium strontium calcium descaling and blockage relieving agent and preparation method thereof that the invention discloses a kind of near wellbore zone, including polyamine carboxylic acid salt solution, accounts for the nonionic surface active agent of polyamine carboxylic acid salt solution gross mass 3%~10% and account for the demulsifier of polyamine carboxylic acid salt solution gross mass 2%~8%；The polyamine carboxylic acid salt solution is 1.05~1.5 by molar ratio:Polyamine intermediate made of 1 organic amine and epichlorohydrin reaction reacts manufactured chloracetate reaction with the chloroethene bronsted lowry acids and bases bronsted lowry of equimolar amounts and is prepared；The barium strontium calcium descaling and blockage relieving agent of the near wellbore zone has good elimination effect, descaling rate to difficulty soluble salts such as barium sulfate, strontium sulfate, calcium sulfate>40%；Meanwhile should have and prevent swollen rejection, clay swell reduced rate rate>80%, it is slight to the corrosivity of equipment, and water will not be caused to lock.Reservoir permeability can be improved, and then improve the recovery ratio of petroleum resources effectively to nearly well reservoir blockages relieving.
Description
Technical field
The present invention relates to a kind of descaling and blockage relieving agent and preparation method thereof for oil field near wellbore zone, more particularly to a kind of use
In the calcium sulfate in oil field, the descaling and blockage relieving agent and preparation method thereof of strontium sulfate, barium sulfate.
Background technology
In the development process of petroleum resources, the method for recovery ratio each elephant at home extensively is improved using water filling
Using.Since the water and reservoir noted contain abundant Ca in the middle2+、Ba2+、Sr2+Deng cation and SO4 2-Anion, when this
Cationoid and anion will generate the difficulty soluble salts such as calcium sulfate, barium sulfate, strontium sulfate when meeting, and cause in water filling stratum, oil
There is Structure Phenomenon in casing, gathering line, ground installation, seriously affect the exploitation of petroleum resources.In addition, because of most of brill
Well liquid is mostly aggravated using barite, is easy to cause pore plugging in the near wellbore zone of reservoir, especially in horizontal well drilling process
In, this phenomenon is particularly acute.The conventional method for solving the problem of this, which is pickling, but pickling is brought is corroded to equipment
Seriously, and since acid cannot dissolve the inorganic salts such as calcium sulfate, barium sulfate, strontium sulfate.Undissolved calcium sulfate, barium sulfate, sulfuric acid
The inorganic particles such as strontium are easy to cause secondary injury to reservoir.
Two approach to solve the above problems are：(1) formation and aggregation of calcium sulfate, barium sulfate, strontium sulfate etc. are prevented；
(2) to established dirty or pore plugging is purged and de-plugging.Existing patent report is mostly the first approach.It discloses specially
Sharp CN201110314543.7 has invented a kind of Barium-Strontium Sulfate Scale Retarder, contains poly- epoxy succinic hydrochloric acid, polyamines Quito ether first
Pitch phosphonic acids, ZG-558 antisludging agents (being copolymerized by maleic anhydride, hydroxypropyl acrylate, sodium hypophosphite), polyquaternium, water etc.
Ingredient.Mechanism is to prevent it to be contacted with sulfate radical by divalent ions such as chelating agent complexing calcium, strontium, barium and generate indissoluble inorganic salts,
And prevent the formation of incrustation scale by preventing the modes such as difficulty soluble salt crystal accumulation growth；Publication
CN201210404432.X, CN201210408497.1, CN201210484135.0 etc. disclose antisludging agent scale-inhibiting properties and
The test method of influence factor；But this approach can only slow down fouling, cannot thoroughly inhibit.Therefore, it is also desirable to have second
Approach.It is reported about the invention of scale remover at present, the publication applied such as Xi'an Petroleum University
CN201410097184.8 is related to a kind of barium sulfate, strontium sulfate scale remover and preparation method thereof, and the host agent of formula is that one kind contains
Nitrogen polybasic carboxylic acid.In addition, publication CN201210480955.2, CN201210478949.3, CN201210480940.6,
CN201210484037.7、CN201210484180.6、CN201210483230.9、CN201210486464.9、
CN201210486482.7 etc. discloses the influence factor of scale remover and the test method of performance.
Invention content
The purpose of the present invention is to provide it is a kind of in oil field containing components such as calcium sulfate, barium sulfate, strontium sulfates
The removing of incrustation scale and caused by heavy weight additive barium sulfate reservoir block de-plugging the barium strontium calcium descaling and blockage relieving near wellbore zone
Agent.
The use for having both descaling and blockage relieving and inhibiting clay swelling function is prepared another object of the present invention is to provide a kind of
In the preparation method of the barium strontium calcium descaling and blockage relieving agent of near wellbore zone.
To achieve the goals above, the barium strontium calcium descaling and blockage relieving agent near wellbore zone of the invention, including polyamine carboxylic acid
Salting liquid accounts for the nonionic surface active agent surface-active of polyamine carboxylic acid salt solution gross mass 3%~10% and accounts for polyamine carboxylic
The demulsifier of acid salt solution gross mass 2%~8%；The polyamine carboxylic acid salt solution is 1.05~1.5 by molar ratio:1 it is organic
The chloracetate that amine and epoxychloropropane are blended standby polyamine intermediate with the chloroethene bronsted lowry acids and bases bronsted lowry of equimolar amounts is mixed with reacts
It is prepared, the molar ratio of the monoxone and the organic amine is 2.5~5:1.
A kind of preparation method of barium strontium calcium descaling and blockage relieving agent near wellbore zone, includes the following steps：
(1) polyamine is prepared：
Under room temperature, organic amine is dissolved in the water of 1~2 times of quality, ice-water bath temperature control, stirs while ring is slowly added dropwise
The molar ratio of oxygen chloropropane, the organic amine and the epoxychloropropane is 1.05~1.5:1, restore to room temperature after completion of dropwise addition
Under the conditions of continue 1~2h of stirring, then heat to 50 DEG C~70 DEG C stirring 3~5h, stop heating, be cooled to room temperature to get to
Polyamine midbody solution；
(2) polyamine carboxylate is prepared：
In 1~5 DEG C of temperature range of temperature control, monoxone is dissolved in the water of 2 times of quality, in the monoxone and step (1)
The molar ratio of the organic amine is 2.5~5:1, stirring simultaneously be slowly added dropwise with the aqueous slkali of monoxone equimolar amounts or be slightly more than
The aqueous slkali of monoxone molal quantity makes the hydrogen ion in the monoxone be overlapped completely by the hydroxide ion in aqueous slkali, system
Corresponding chloracetate solution is obtained, ice-water bath temperature control, control reacting liquid temperature is used to be no more than 30 DEG C of (reaction temperatures in reaction process
It can float between 5~30 DEG C)；
Obtained chloracetate solution is added in step (1) and is made in polyamine midbody solution, stirs 10 at room temperature
Then~20min is added dropwise aqueous slkali and adjusts pH value of solution to 10~12, then between being warming up to 50~60 DEG C 4~6h of reaction to get to
Polyamine carboxylic acid salt solution；
(3) descaling and blockage relieving agent is prepared：
It is added in the polyamine carboxylic acid salt solution made from step (2) and accounts for polyamine carboxylic acid salt solution gross mass 3%~10%
Nonionic surface active agent surfactant and the demulsifier for accounting for polyamine carboxylic acid salt solution gross mass 2%~8%, stirring 15~
30min is to being uniformly mixed to get to barium strontium calcium descaling and blockage relieving agent.
The organic amine in step (1) is ethylenediamine, diethylenetriamine or triethylene tetramine.
The aqueous slkali in step (2) is the sodium hydroxide solution of 30wt% or the potassium hydroxide solution of 30wt%.
The nonionic surface active agent in step (3) is alkyl phenol polyoxyethylene ether class non-ionic surfactant
Agent or fatty alcohol polyethenoxy ether class nonionic surface active agent.
Preferably, the alkyl phenol polyoxyethylene ether class nonionic surface active agent is OP-7 or OP-9.
Preferably, the fatty alcohol polyethenoxy ether class nonionic surface active agent is AEO-7 or AEO-9.
The demulsifier in step (3) is AP types demulsifier and AE type demulsifiers.
Preferably, the AP types demulsifier is AP8051, AP212, AP134 or AP136 demulsifier.
Preferably, the AE types demulsifier is AE1910, AE9901 type, AE0604, AE31 or AE8031.
With the polyamine multi-carboxylate with extremely strong sequestering power in the barium strontium calcium descaling and blockage relieving agent prescription of the near wellbore zone
For host agent, the indissolubles inorganic salts such as calcium sulfate, barium sulfate, strontium sulfate are dissolved under alkaline condition, and prevent swollen inhibition with superior
Ability and dispersibility play and inhibit clay swell migration in stratum, indissoluble inorganic salts is prevented to assemble fouling, substantially reduce scale removal
Secondary injury of the agent to reservoir；In addition, further preferably surfactant and demulsifier in formula, its role is on the one hand can
The oil slick for cleaning incrustation scale surface is conducive to being in direct contact for chelating agent and incrustation scale；On the other hand it can prevent from removing in the construction process
Dirty agent causes reservoir water to lock；Be conducive to the dispersion of solia particle without coagulation simultaneously.
The barium strontium calcium descaling and blockage relieving agent of the near wellbore zone has the difficulty soluble salts such as barium sulfate, strontium sulfate, calcium sulfate good
Elimination effect, descaling rate>40%；Meanwhile should have and prevent swollen rejection, clay swell reduced rate rate>80%, the corruption to equipment
Corrosion is slight, and water will not be caused to lock.Reservoir permeability can be improved, and then improve oil gas money effectively to nearly well reservoir blockages relieving
The recovery ratio in source.
Specific implementation mode
The foregoing invention content of the present invention is described in further detail With reference to embodiment.But it should not incite somebody to action
This range for being interpreted as the above-mentioned theme of the present invention is only limitted to following embodiments.The above-mentioned technological thought situation of the present invention is not being departed from
Under, according to ordinary skill knowledge and customary means, various replacements and change are made, the scope of the present invention should all be included in
It is interior.
Embodiment 1
(1) preparation of polyamine:
At ambient temperature, 50mL triethylene tetramines are dissolved in the water of 50mL, in the case of ice-water bath and stirring slowly
24.9g epoxychloropropane is added dropwise, and controlling reaction temperature is restored after completion of dropwise addition to room temperature at 5~30 DEG C during dropwise addition
Under the conditions of continue to stir 1h, then heat to 60 DEG C and continue to stir 4h, stop heating, be cooled to room temperature, polyamine intermediate is made；
(2) preparation of polyamine carboxylate：
109g monoxones are dissolved in 2 DEG C of ice water of 218g, ice-water bath temperature control, stirring is slowly added to 154g thereto simultaneously
The sodium hydroxide solution that mass fraction is 30%, control reacting liquid temperature are no more than 30 DEG C, and sodium chloroacetate solution is made in reaction
It is added to step (1) to be made in polyamine solution, stirs 10min, the sodium hydroxide solution that mass fraction is 30% is then used to adjust
PH value of solution is to 12, then is warming up to 50 DEG C of reaction 6h, and polyamine carboxylic acid salt solution is made；
(3) preparation of descaling and blockage relieving agent
50g fatty alcohol polyethenoxy ether class surfactants are added in the polyamine carboxylic acid salt solution made from step (2)
AEO-9 and 40g AP type demulsifier AP212 are uniformly mixed and obtain the barium strontium calcium descaling and blockage relieving agent of the near wellbore zone.
Embodiment 2
(1) preparation of polyamine:
At ambient temperature, 50mL diethylenetriamines are dissolved in the water of 100mL, in the case of ice-water bath and stirring slowly
40g epoxychloropropane is added dropwise, and controlling reaction temperature is restored after completion of dropwise addition to room temperature item at 5~30 DEG C during dropwise addition
Continue to stir 1h under part, then heats to 60 DEG C and continue to stir 5h, stop heating, be cooled to room temperature, polyamine intermediate is made；
(2) preparation of polyamine carboxylate：
172g monoxones are dissolved in 2 DEG C of ice water of 344g, ice-water bath temperature control, stirring is slowly added to 242g thereto simultaneously
The sodium hydroxide solution that mass fraction is 30%, control reacting liquid temperature are no more than 30 DEG C, and sodium chloroacetate solution is made in reaction
It is added to step (1) to be made in polyamine solution, stirs 10min, the sodium hydroxide solution that mass fraction is 30% is then used to adjust
PH value of solution is to 10, then is warming up to 60 DEG C of reaction 4h, and polyamine carboxylic acid salt solution is made；
(3) preparation of descaling and blockage relieving agent：
20g fatty alcohol polyethenoxy ether class surfactants are added in the polyamine carboxylic acid salt solution made from step (2)
AEO-7,20g AE type demulsifier AE0604 are uniformly mixed and obtain the barium strontium calcium descaling and blockage relieving agent of the near wellbore zone.
Embodiment 3
(1) preparation of polyamine:
At ambient temperature, 50mL diethylenetriamines are dissolved in the water of 100mL, in the case of ice-water bath and stirring slowly
40g epoxychloropropane is added dropwise, and controlling reaction temperature is restored after completion of dropwise addition to room temperature item at 5~30 DEG C during dropwise addition
Continue to stir 1h under part, then heats to 60 DEG C and continue to stir 5h, stop heating, be cooled to room temperature, polyamine intermediate is made；
(2) preparation of polyamine carboxylate：
108g monoxones are dissolved in 2 DEG C of ice water of 216g, ice-water bath temperature control, stirring is slowly added to 152g thereto simultaneously
The sodium hydroxide solution that mass fraction is 30%, control reacting liquid temperature are no more than 30 DEG C, and sodium chloroacetate solution is made in reaction
It is added to step (1) to be made in polyamine solution, stirs 10min, the sodium hydroxide solution that mass fraction is 30% is then used to adjust
PH value of solution is to 11, then is warming up to 60 DEG C of reaction 4h, and polyamine carboxylic acid salt solution is made；
(3) preparation of descaling and blockage relieving agent：
25g alkyl phenol polyoxyethylene ether classes Surfactant OP-is added in the polyamine carboxylic acid salt solution made from step (2)
7,24g AP types demulsifier AP134 is uniformly mixed and obtains the barium strontium calcium descaling and blockage relieving agent of the near wellbore zone.
Performance test：
(1) descaling and blockage relieving performance test：
Descaling and blockage relieving performance test methods are as follows：
(1) descaling and blockage relieving agent in embodiment is configured to the aqueous solution that mass fraction is 50%, 100g has been configured
Descaling and blockage relieving agent aqueous solution is placed in the wide-mouth bottle that can be sealed, and adds 10g barium sulfate, and magneton is added and seals；
(2) it utilizes 50 DEG C or 80 DEG C of oil bath temperature control and heats under magnetic stirring for 24 hours or 48h postcoolings are to room temperature；
(3) it is m to take a filter paper, weighing quality1, reaction solution after cooling is filtered, and constantly clean filter cake with clear water, so
Filter cake and filter paper are dried afterwards, after drying, the quality for weighing filter paper and filter cake is m2；
(4) descaling and blockage relieving efficiency (f) calculates：
Calculation formula：F=[1- (m2-m1)/10] * 100%；
Test result is as follows shown in table 1.
Table 1：
By data in upper table 1 it is found that the descaling and blockage relieving agent of the present invention recycles 2 days can meet scale removal at a temperature of 80 DEG C
It needs, realizes 40% or more de-plugging efficiency.
(2) prevent swollen rejection test：
Prevent that swollen rejection test method is as follows：
(1) 0.50g bentonite in powder is weighed, is fitted into 10mL centrifuge tubes, the embodiment that 10mL mass fractions are 10% is added
Solution fully shakes up, and places 2h at room temperature, is packed into centrifuge, centrifuges 15min in the case where rotating speed is 1500r/min, surveys
Go out the intumescent system V of bentonite in powder1；
(2) step (1) is repeated, with the aqueous solution for the embodiment that 10mL deionized waters substitution mass fraction is 10%, is measured
The swelling volume V of bentonite in powder in deionized water2；
(3) step (1) is repeated, with the aqueous solution for the embodiment that 10mL kerosene substitution mass fraction is 10%, measures swelling
The swelling volume V of native powder in deionized water0；
(4) anti-dilative B (%) is calculated：Anti-dilative is calculated by following formula：
B=(V2-V1)/(V2-V0) * 100%；
The test result is as shown in table 2.
Table 2：Descaling and blockage relieving agent tests the anti-dilative of clay
| Test product | Anti-dilative |
| The aqueous solution of 10wt% embodiments 1 | 85% |
| The aqueous solution of 10wt% embodiments 2 | 89% |
| The aqueous solution of 10wt% embodiments 3 | 83% |
By data in table 2 it is found that the descaling and blockage relieving agent of the present invention has anti-clayswelling rejection, it effectively prevent scale removal solution
Blocking agent causes clay swell that reservoir pore space is caused to block in practical applications.
(3) Evaluation of Corrosion Resistance
Evaluation of Corrosion Resistance is carried out to product prepared by Examples 1 to 3, test method refers to professional standard SY/
T0026-1999, wherein the test steel that steel are that grade of steel is N80, test temperature are 80 DEG C, and test result is as shown in table 3.
Table 3：The erosion analysis of scale remover
| Test product | Corrosion rate (mm/a) | Evaluation |
| The aqueous solution of 50wt% embodiments 1 | 0.02735 | Mild corrosion |
| The aqueous solution of 50wt% embodiments 2 | 0.02846 | Mild corrosion |
| The aqueous solution of 50wt% embodiments 3 | 0.02659 | Mild corrosion |
The descaling and blockage relieving agent of the present invention only has slight erosion to steel it can be seen from data in table 3, can expire completely
Sufficient underground construction requirement.
Above-described embodiment and respective performances test are only the explanations to product of the present invention, not make any shape to the present invention
Limitation in formula, within the scope of not departing from technical solution of the present invention, any technology contents using the disclosure above are made simply
The equivalent program of transformation, belongs to protection scope of the present invention.
Claims (10)
1. a kind of preparation method of barium strontium calcium descaling and blockage relieving agent near wellbore zone, which is characterized in that include the following steps：
(1) polyamine is prepared：
Under room temperature, organic amine is dissolved in the water of 1~2 times of quality, ice-water bath temperature control, stirs while epoxy chlorine is slowly added dropwise
The molar ratio of propane, the organic amine and the epoxychloropropane is 1.05~1.5:1, restore to room temperature condition after completion of dropwise addition
Under continue 1~2h of stirring, then heat to 50 DEG C~70 DEG C 3~5h of stirring, stop heating, be cooled to room temperature to get to polyamine
Midbody solution；
(2) polyamine carboxylate is prepared：
At a temperature of 1~5 DEG C, monoxone is dissolved in the water of 2 times of quality, the monoxone and organic amine described in step (1)
Molar ratio be 2.5~5:1, the aqueous slkali with monoxone equimolar amounts is stirred while being slowly added dropwise, chloracetate solution is made,
Obtained chloracetate solution is added in step (1) and is made in polyamine midbody solution, stirs 10~20min at room temperature,
Then aqueous slkali is added dropwise and adjusts pH value of solution to 10~12, then between being warming up to 50~60 DEG C 4~6h of reaction to get to polyamine carboxylic acid
Salting liquid；
(3) descaling and blockage relieving agent is prepared：
In the polyamine carboxylic acid salt solution made from step (2) be added account for polyamine carboxylic acid salt solution gross mass 3%~10% it is non-from
Subtype surfactant and the demulsifier for accounting for polyamine carboxylic acid salt solution gross mass 2%~8%, 15~30min of stirring are equal to mixing
It is even to get to barium strontium calcium descaling and blockage relieving agent.
2. the preparation method of the barium strontium calcium descaling and blockage relieving agent according to claim 1 near wellbore zone, which is characterized in that
The organic amine in step (1) is ethylenediamine, diethylenetriamine or triethylene tetramine.
3. the preparation method of the barium strontium calcium descaling and blockage relieving agent according to claim 1 near wellbore zone, which is characterized in that
The aqueous slkali in step (2) is the sodium hydroxide solution of 30wt% or the potassium hydroxide solution of 30wt%.
4. the preparation method of the barium strontium calcium descaling and blockage relieving agent according to claim 1 near wellbore zone, which is characterized in that
The nonionic surface active agent in step (3) is alkyl phenol polyoxyethylene ether or fatty alcohol polyoxyethylene ether.
5. the preparation method of the barium strontium calcium descaling and blockage relieving agent according to claim 4 near wellbore zone, which is characterized in that
The alkyl phenol polyoxyethylene ether class nonionic surface active agent is OP-7 or OP-9.
6. the preparation method of the barium strontium calcium descaling and blockage relieving agent according to claim 4 near wellbore zone, which is characterized in that
The fatty alcohol polyethenoxy ether class nonionic surface active agent is AEO-7 or AEO-9.
7. the preparation method of the barium strontium calcium descaling and blockage relieving agent according to claim 1 near wellbore zone, which is characterized in that
The demulsifier in step (3) is AP types demulsifier and AE type demulsifiers.
8. the preparation method of the barium strontium calcium descaling and blockage relieving agent according to claim 7 near wellbore zone, which is characterized in that
The AP types demulsifier is AP8051, AP212, AP134 or AP136.
9. the preparation method of the barium strontium calcium descaling and blockage relieving agent according to claim 7 near wellbore zone, which is characterized in that
The AE types demulsifier is AE1910, AE9901, AE0604, AE31 or AE8031.
10. a kind of preparation side of such as barium strontium calcium descaling and blockage relieving agent according to any one of claims 1 to 9 near wellbore zone
Barium strontium calcium descaling and blockage relieving agent near wellbore zone prepared by method.
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| CN108005615A (en) * | 2017-11-22 | 2018-05-08 | 中国石油集团渤海钻探工程有限公司 | A kind of de-plugging construction technology for being used to release the pollution of barium strontium calcium compound scale |
| CN109575894B (en) * | 2018-12-29 | 2020-04-21 | 黑龙江益瑞化工有限公司 | Neutral blocking remover for chemical oil extraction in oil field and preparation method thereof |
| CN114085659A (en) * | 2020-08-24 | 2022-02-25 | 中国石油天然气股份有限公司 | Descaling blocking remover for high-temperature and high-pressure oil and gas wells and preparation method thereof |
| CN112094633A (en) * | 2020-10-29 | 2020-12-18 | 四川中汇安达石油化工有限公司 | Chelating type blocking remover and preparation method and application thereof |
| CN117384611B (en) * | 2023-12-13 | 2024-02-13 | 东营煜煌能源技术有限公司 | Solid descaling blocking remover and preparation method thereof |
| CN117511527B (en) * | 2024-01-02 | 2024-03-19 | 东营煜煌能源技术有限公司 | Descaling blocking remover and preparation method thereof |
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